ASTM C25-99
(Test Method)Standard Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated Lime
Standard Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated Lime
SCOPE
1.1 These test methods cover the chemical analysis of high-calcium and dolomitic limestone, quicklime, and hydrated lime. These test methods are classified as either standard (preferred) or alternative (optional).
1.2 The standard test methods are those that employ classical gravimetric or volumetric analytical procedures and are typically those required for referee analyses where chemical specification requirements are an essential part of contractual agreement between buyer and seller.
1.3 Alternative or optional test methods are provided for those who wish to use procedures shorter or more convenient than the standard methods for the routine determinations of certain constituents. Optional test methods may sometimes be preferred to the standard test methods, but frequently the use of modern and expensive instrumentation is indicated which may not be accessible to everyone. Therefore, the use of these test methods must be left to the discretion of each laboratory.
1.4 The analytical procedures appear in the following order: Section Aluminum Oxide 15 Available Lime Index 28 Calcium and Magnesium Oxide: Alternative EDTA Titration Method 31 Calcium Carbonate Equivalent 33 Calcium Oxide: Gravimetric Method 16 Volumetric Method 17 Carbon Dioxide by Standard Method 22 Combined Oxides of Iron and Aluminum 12 Ferrous Iron X5 Free Calcium Oxide X6 Free Moisture in Hydrated Lime 21 Free Moisture in Limestone 20 Free Silica 29 Insoluble Matter Including Silicon Dioxide: Standard Method 8 Optional Perchloric Acid Method 9 Insoluble Matter Other Than Silicon Dioxide 11 Loss on Ignition 19 Magnesium Oxide 18 Manganese: Bismuthate Method X4 Periodate (Photometric) Method 27 pH Determination of Alkaline Earth Solutions 34 1a Phosphorus: Titrimetric Method X3 Molybdovanadate Method 26 Silicon Dioxide 10 Strontium Oxide X2 Sulfur Trioxide 23 Total Carbon: Direct Combustion-Thermal Conductivity Cell Method 32 Total Iron: Standard Method, Potassium Dichromate Titration 13 Potassium Permanganate Titration Method X1 Ortho-Phenanthroline, Photometric Method 14 Total Sulfur: Sodium Carbonate Fusion 24 Combustion-Iodate Titration Method 25 Unhydrated Oxides 30
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Notes 11, 13, 27, 47, X2.1, and X5.1.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:C 25–99
Standard Test Methods for
Chemical Analysis of Limestone, Quicklime, and Hydrated
Lime
ThisstandardisissuedunderthefixeddesignationC25;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
Manganese:
Bismuthate Method Appendix X4
1.1 These test methods cover the chemical analysis of
Periodate (Photometric) Method 27
high-calcium and dolomitic limestone, quicklime, and hy-
pH Determination of Alkaline Earth Solu- 34
tions
dratedlime.Thesetestmethodsareclassifiedaseitherstandard
Phosphorus:
(preferred) or alternative (optional).
Titrimetric Method Appendix X3
1.2 The standard test methods are those that employ classi-
Molybdovanadate Method 26
Silicon Dioxide 10
cal gravimetric or volumetric analytical procedures and are
Strontium Oxide Appendix X2
typically those required for referee analyses where chemical
Sulfur Trioxide 23
specification requirements are an essential part of contractual Total Carbon:
Direct Combustion-Thermal Conductiv- 32
agreement between buyer and seller.
ity Cell Method
1.3 Alternative or optional test methods are provided for
Total Carbon and Sulfur:
those who wish to use procedures shorter or more convenient Combustion/Infrared Detection Method 35
Total Iron:
than the standard methods for the routine determinations of
Standard Method, Potassium Dichro- 13
certain constituents. Optional test methods may sometimes be
mate Titration
Potassium Permanganate Titration Appendix X1
preferredtothestandardtestmethods,butfrequentlytheuseof
Method
modern and expensive instrumentation is indicated which may
Ortho-Phenanthroline, Photometric 14
not be accessible to everyone. Therefore, the use of these test
Method
Total Sulfur:
methods must be left to the discretion of each laboratory.
Sodium Carbonate Fusion 24
1.4 The analytical procedures appear in the following order:
Combustion-Iodate Titration Method 25
Section
Unhydrated Oxides 30
Aluminum Oxide 15
Available Lime Index 28 1.5 This standard does not purport to address all of the
Calcium and Magnesium Oxide:
safety concerns, if any, associated with its use. It is the
Alternative EDTATitration Method 31
responsibility of the user of this standard to establish appro-
Calcium Carbonate Equivalent 33
Calcium Oxide: priate safety and health practices and determine the applica-
Gravimetric Method 16
bility of regulatory limitations prior to use. For specific
Volumetric Method 17
precautionary statements, see Note 11, Note 13, Note 27, Note
Carbon Dioxide by Standard Method 22
Combined Oxides of Iron and Aluminum 12 51, Note X2.1, and Note X5.1.
Ferrous Iron Appendix X5
Free Calcium Oxide Appendix X6
2. Referenced Documents
Free Moisture in Hydrated Lime 21
Free Moisture in Limestone 20 2.1 ASTM Standards:
Free Silica 29
C 50 Practice for Sampling, Inspection, Packing, and Mark-
Insoluble Matter Including Silicon Dioxide:
ing of Lime and Limestone Products
Standard Method 8
Optional Perchloric Acid Method 9 C51 Terminology Relating to Lime and Limestone (as
Insoluble Matter Other Than Silicon Diox- 11
Used by the Industry)
ide
C911 Specification for Quicklime, Hydrated Lime, and
Loss on Ignition 19
Magnesium Oxide 18
Limestone for Chemical Uses
D 1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to
ThesetestmethodsareunderthejurisdictionofASTMCommitteeC-7onLime
and are the direct responsibility of Subcommittee C07.05 on Chemical Tests.
Current edition approved Aug. 10, 1999. Published September 1999. Originally Annual Book of ASTM Standards, Vol 04.01.
published as C 25–19T. Last previous edition C 25–98. Annual Book of ASTM Standards, Vol 11.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C25–99
Determine Conformance with Specifications alloy not requiring protective coating and shall meet the
E 50 Practices for Apparatus, Reagents, and Safety Precau- density requirements for Class S.
tions for Chemical Analysis of Metals 5.1.3 Glassware and Laboratory Containers—Standard
E70 Test Method for pH of Aqueous Solutions with the volumetric flasks, burets, pipets, dispensers, etc., shall be
Glass Electrode carefully selected precision grade or better and shall be
E 173 Practice for Conducting Interlaboratory Studies of calibrated, if necessary, to meet the requirements of each
Methods for Chemical Analysis of Metals operation. Standard-type interchangeable ground glass orTFE-
E 200 Practice for Preparation, Standardization, and Stor- fluorocarbon joints are recommended for all volumetric glass-
age of Standard and Reagent Solutions for Chemical ware. Polyethylene containers are recommended for all aque-
Analysis ous solutions of alkalies and for standard solutions where the
E 691 Practice for Conducting an Interlaboratory Study to presence of dissolved silica or alkali from the glass would be
Determine the Precision of a Test Method objectionable.
E 832 Specification for Laboratory Filter Papers 5.1.4 Desiccators—Desiccators shall be provided with a
good desiccant such as anhydrous magnesium perchlorate,
3. Terminology
activated alumina, sulfuric acid, or phosphoric anhydride.
3.1 Definitions—Unless otherwise specified, for definitions Anhydrous calcium sulfate may also be used provided it has
of terms used in these test methods refer to TerminologyC51. been treated with a color-changing indicator to show when the
desiccant has lost its effectiveness. Calcium chloride and silica
4. Significance and Use
gel are not satisfactory desiccants for this type of analysis.
4.1 These test methods provide accurate and reliable ana- 5.1.5 Filter Paper—Filter paper shall conform to the re-
lytical procedures to determine the chemical constituents of
quirements of SpecificationE 832,Type II (quantitative). Class
limestone, quicklime, and hydrated lime (Note 1).The percent- E shall be used for coarse and gelatinous precipitates. When
ages of specific constituents which determine a material’s
medium-textured paper is required, Class F filter paper shall be
qualityorfitnessforuseareofsignificancedependinguponthe used. When a retentive paper is needed, Class G shall be used.
purpose or end use of the material. Results obtained may be
Recommendations: Filter Pore Size Filter Speed
Class (microns)
used in relation to specification requirements.
E 20 to 25 fast speed
4.2 Because quicklime and hydrated lime quickly absorb
F 8 medium speed
water and carbon dioxide from the air, precision and bias are
G 2.5 slow speed
extremely dependent upon precautions taken during sample
5.1.6 Crucibles—Platinum crucibles and tight fitting lids
preparation and analysis to minimize excessive exposure to
should preferably be made of pure unalloyed platinum and be
ambient conditions.
of 25 to 35-mL capacity. Where alloyed platinum is used for
NOTE 1—These test methods can be applied to other calcareous
greater stiffness or to obviate sticking of fused material to
materials if provisions are made to compensate for known interferences.
crucible or lid, the alloyed platinum should not decrease in
weight by more than 0.2 mg when heated at 1200°C for 1 h.
5. General Apparatus and Materials and Reagents
5.1.7 Muffle Furnace—The electric muffle furnace should
5.1 General Apparatus and Materials:
be capable of continuous operation up to 1000°C and be
5.1.1 Balance—The balance shall be of an analytical type
capable of intermittent operation at higher temperatures if
with a capacity not to exceed 200 g. It may be of conventional
required. It should have an indicating pyrometer accurate to
design or it may be a constant-load, direct-reading type. It shall
625°C.
be capable of reproducing weighings within 0.0002 g with an
5.2 Reagents:
accuracy of 60.0002 g. Rapid weighing devices that may be
5.2.1 Purity of Reagents—Reagent grade chemicals shall be
provided such as a chain, damper, or heavy riders shall not
used in all tests. Unless otherwise indicated, it is intended that
increase the basic inaccuracy by more than 0.0001 g at any
all reagents shall conform to the specifications of the Commit-
reading and with any load within the rated capacity of the
tee onAnalytical Reagents of theAmerican Chemical Society
balance.
where such specifications are available. Other grades may be
5.1.2 Weights—Weights used for analysis shall conform to
used provided it is first ascertained that the reagent is of
Class S-1 requirements of the National Institute of Standards
sufficiently high purity to permit its use without lessening the
andTechnologyasdescribedinNISTCircular547. Theyshall
accuracy of the determination. In addition to this, it is desirable
be checked at least once a year or when questioned, and
in many cases for the analyst to ensure the accuracy of his
adjusted to within allowable tolerances for Class S-1 weights.
results by running blanks or checking against a comparable
All new sets of weights purchased shall have the weights of 1
sample of known composition.
g and larger made of stainless steel or other corrosion-resistant
4 9
Annual Book of ASTM Standards, Vol 14.02. Reagent Chemicals, American Chemical Society Specifications, American
Annual Book of ASTM Standards, Vol 03.05. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Discontinued 1997; see 1997 Annual Book of ASTM Standards, Vol 03.05. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 15.05. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Available from National Institute of Standards and Technology, Gaithersburg, and National Formulary, U.S. Pharmacopeia Convention, Inc. (USPC), Rockville,
MD 20899. MD.
C25–99
5.2.2 Purity of Water—Unless otherwise indicated, refer- 6.4.1 The calculations included in the individual procedures
ences to water are understood to mean distilled water or other sometimes assume that the exact weight specified has been
water of equivalent purity. Water conforming to Specification used. Accurately weighed samples which are approximately
D 1193 meets these requirements. but not exactly equal to the weight specified may be used
provided appropriate corrections are made in the calculation.
5.2.3 Concentration of Reagents:
Unless otherwise stated, weights of all samples and residues
5.2.3.1 Concentrated Acids and Ammonium Hydroxide—
should be recorded to the nearest 0.0001 g.
When acids and ammonium hydroxide are specified by name
6.4.2 In all mathematical operations on a set of observed
or chemical formula only, it shall be understood that concen-
values, the equivalent of two more places of figures than in the
trated reagents approximating the following specific gravities
single observed values shall be retained. For example, if
or concentrations are intended:
observed values are read or determined to the nearest 0.1 mg,
Acetic acid (HC H O ) 99.5 %
2 3 2
Hydrochloric acid (HCl) sp gr 1.19 carry numbers to the nearest 0.001 mg in calculation.
Hydrofluoric acid (HF) 48 %
6.5 Rounding Figures—Rounding figures to the nearest
Nitric acid (HNO ) sp gr 1.42
significant place required in the report should be done after the
Perchloric acid (HClO)70%
Phosphoric acid (H PO)85% calculations are completed, in order to keep the final results
3 4
Sulfuric acid (H SO ) sp gr 1.84
2 4
free from calculation errors. The rounding procedure should
Ammonium hydroxide (NH OH) sp gr 0.90
follow the principle outlined in PracticeE29.
5.2.3.2 Dilute Reagents—The concentration of dilute acids
7. Performance Requirements for Test Methods
and NH OH except when standardized, are specified as a ratio
stating the number of measured volumes of the concentrated
7.1 Referee Analyses—The reference test methods that ap-
reagenttobedilutedwithagivennumberofmeasuredvolumes
pear in Sections 8 through 32, or any other test methods
of water. In conformance with international practice, new and
qualified in accordance with 7.3, are required for referee
revised methods will use the “plus” designation instead of the
analysis in those cases where conformance to the requirements
ratio (:) symbol as the specified designation of dilution; for
of a chemical specification are questioned. In these cases a
example, H SO (5 + 95) means 5 volumes of concentrated
2 4 limestone, quicklime, or hydrated lime shall not be rejected for
H SO (sp gr 1.84) diluted with 95 volumes of water.
2 4 failure to conform to chemical requirements unless all sample
5.2.3.3 Standard Solutions—Concentrations of standard so-
preparationandanalysisofanyoneconstituentismadeentirely
lutions shall be expressed as normalities (N) or as equivalents
byreferencetestmethodsprescribedintheappropriatesections
in grams per millilitre of the component to be determined, for
of this test method or by other qualified test methods. Excep-
example: 0.1 N K Cr O solution (1 mL = 0.004 g Fe O ).The
tion can be made when specific test methods are prescribed in
2 2 7 2 3
average of at least three determinations shall be used for all
the standard specification for the limestone, quicklime, or
standardizations. The standardization used to determine the
hydrated lime in question. The test methods actually used for
strength of the standard solutions is described in the text under
the analysis shall be designated.
each of the appropriate procedures.
7.1.1 Whenthereisaquestionregardingacceptance,referee
analyses shall be made in duplicate. If the two results do not
6. General Procedures agree within the permissible variation given in Table 1, the
determination including sample preparation shall be repeated
6.1 Sampling—Samples of lime and limestone for chemical
analysis shall be taken and prepared in accordance with the
requirements of Methods C 50 applicable to the material to be
A
TABLE 1 Maximum Permissible Variations in Results
tested.
(Column 3)
6.2 Tared or Weighed Crucibles—The tare weight of cru-
Maximum Difference of
(Column 2) the Average of Duplicates
cibles shall be determined by preheating the empty crucible to
(Column 1) Maximum Difference from SRM Certificate
constant weight at the same temperature and under the same
B
Constituent Between Duplicates Values
conditionsasshallbeusedforthefinalignitionofaresidueand
Al as Al O 0.20 60.30
2 3
cooling in a desiccator for the same period of time used for the
Ca as CaO 0.20 60.30
crucible containing the residue. Mg as M
...
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